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Procedure for the preparation of aromatic derivatives of titanoceneCM Patents

[0001] Procedure for the preparation of aromatic derivatives of titanocene, useful as catalysts for the polymerisation and hydrogenation of polymers, characterised by the use of a Grignard reagent. This procedure allows to easily prepare compounds with the general formula : <img class="EMIRef" id="584493293-ia01" /> where: L, which can be equal to or different one from the other, are cyclopentadiene, or pentamethylcyclopentadiene; preferably at least one L is cyclopentadiene; R<1>, R<2>, R<3>, equal or different from one another, are selected from the group consisting of: hydrogen, alkyl group from 1 to 4 carbon atoms, OR<4> where R<4> is an alkyl group of 1 to 4 carbon atoms; at least one of the R<1>, R<2> or R<3> is hydrogen. The preparation is carried out by the reaction of the titanocene dichloride with the corresponding Grignard reagent. This method substantially enhances safety, reproducibility, yield and cost of that carried out via lithium compounds.

Datos clave

CategoríaInvención

Índice de la ficha

Updated at
05/11/2026
Numero publicacion
EP.1072606.A1
Fecha publicacion
31/01/2001
Anio publicacion
2001

En detalle

Reivindicaciones

1. Procedure for the obtaining of a titanonece compound with the following formula: <img class="EMIRef" id="584493295-ib0004" /> where: L, which can be equal or different one from the other, are cyclopentadiene, or pentamethylcyclopentadiene; R<1>, R<2>, R<3>, equal or different one from the other, are selected from the group consisting of: hydrogen, alkyl group of 1 to 4 carbon atoms and OR<4> , where R<4> is an alkyl group of 1 to 4 carbon atoms; at least one of the R<1>, R<2> or R<3> is hydrogen; characterised by the following steps: Preparation of the Grignard reagent by reaction of the magnesium metal with a compound with the formula (II): <img class="EMIRef" id="584493295-ib0005" /> where R<1>, R<2> and R<3> have already been defined and Br is bromine in a polar solvent; Reaction of the Grignard reagent in solution with titanocene dichloride, in a 2:1 ratio; Precipitation with a non-polar solvent, of the chlorobromomagnesium salts generated in the reaction medium and filtration of the same, obtaining a solution of the compound with the formula (I). 2. Procedure according to claim 1 characterised in that at least one L is cyclopentadiene. 3. Procedure according to claims 1-2 where the tianocene compound has the following formula (III): <img class="EMIRef" id="584493295-ib0006" /> where: L, equal or different one from the other, are cyclopentadienyl or pentamethylcyclopentadienyl; OR<4> is an alcoxy group containing from 1 to 4 carbon atoms. 4. Procedure according to claims 1-3, characterised in that solvents used in step a) are liquid with boiling points greater than or equal to 65°C. 5. Procedure according to claims 1-4, characterised in that solvent used in step a) is tetrahydrofuran. 6. Procedure according to claims 1-4, where the synthesised compound is bis(4-methoxy phenyl) bis(cyclopentadienyl) titanium.

Etiquetas

Inventores
Maria Dolores Parellada FerrerFerrer Maria Dolores ParelladaCalle Juan Antonio BarrioJuan Antonio Barrio CalleRoyo Jose SanchoJose Sancho RoyoLuis Mendez LlatasLlatas Luis MendezParellada M DM・D・帕尔拉达弗勒Calle J A Bario巴里奥卡勒锹抟涟Royo J SanchoParallada M D伦壤塔斯Parellada Ferrer, M DoloresParellada Ferrer M DoloresBarrio Calle, Juan AntonioBarrio Calle Juan AntonioSancho Royo, JoseSancho Royo JoseMendez Llatas LuisMendez Llatas, LuisParellada Ferrer, M. Dolores파렐라다페레르,엠에이돌로레스바리오카를,주안안토니오산초로요,호세멘데즈라타스,루이스Parellada Ferrer Maria DoloresParellada Ferrer, Ma DoloresParellada Ferrer Ma DoloresRoyo José Sancho
Solicitantes
Repsol Química S.A.莱比索尔化学股份公司
Clasificacion ipc
C07F 17/ 00 A IC07F 7/ 28 A I
Clasificacion cpc
4H050/AA024H050/AD154H050/AD174H050/BB254H050/BB434H050/BB494H050/BD704H050/WB114H050/WB21C07F17/00502/103502/117526/160526/943556/53
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